KR101523401B1 - Liquid oral composition, and method for improvement in bactericidal activity of cationic bactericidal agent - Google Patents

Abstract

(A) 0.01 to 0.1% by mass of cetylpyridinium chloride (B) 0.02 to 0.3% by mass of sodium lauroyl sarcosine (B) 40 to 100 mol of an average addition mole number of ethylene oxide And the mass ratio of (A) / (B) is 0.3 to 3, and the mass ratio of (C) / ((A) + (B)) is 1.0 to 20. INDUSTRIAL APPLICABILITY According to the present invention, the bactericide penetrates rapidly into the caries biofilm and exerts an excellent sterilizing power against the caries bacteria. In addition, the occurrence of sedimentation and turbidity is suppressed even at low temperature storage, the appearance stability is good, A liquid oral composition which is effective for prevention can be obtained.

Description

TECHNICAL FIELD [0001] The present invention relates to a liquid oral composition, and a method for improving the sterilizing power of a cationic disinfectant. BACKGROUND OF THE INVENTION < RTI ID = 0.0 &

The present invention relates to a composition for liquid oral cavity which is effective for infiltrating a bactericide into a dental caries biofilm in oral cavity and exhibiting an excellent sterilizing power against a cow's organism bacterium and suppressing occurrence of precipitation and turbidity in low temperature preservation and having excellent external stability And a method for improving the sterilizing power of a cationic bactericide.

Background Art [0002] A dental caries is caused by an oral biofilm formed by a carotid bacterium such as Streptococcus mutans or the like in the oral cavity adheres to a tooth surface, and a tooth is demineralized by an acid produced in the biofilm .

Thus, as a means of preventing caries, in the field of liquid oral compositions, means for sterilizing caries causing cariogenes by blending various bactericides is used. Particularly, a cationic fungicide such as benzethonium chloride or cetylpyridinium chloride has a high bactericidal activity against caries bacteria and has a property of being easily adsorbed on the surface of oral tissues such as teeth and oral mucous membranes. Therefore, many oral compositions .

However, these cationic bactericides exhibit a good bactericidal effect against floating bacteria in the oral cavity, but they have a weak penetration into the oral biofilm, and in particular, they exhibit sufficient bactericidal effect against the cariogenic bacteria in the oral biofilm .

Examples of sterilization techniques using a cationic sterilizing agent include oral sterilization techniques using a cationic sterilizing agent such as an adsorption promoting technique by mixing polyphosphoric acid and polyglycerin fatty acid ester (see Patent Document 1), erythritol, xylitol, (Patent Document 2), a technique of suppressing the formation of plaque by mixing palatinit, maltitol and lactitol and inhibiting protein adsorption on the tooth surface (see Patent Document 2), a technology for enhancing tooth adsorption of a bactericide by blending polyvinyl alcohol with a cationic bactericide (Refer to Patent Document 3), a sterilization activity enhancement technology (see Patent Document 4) that improves usability by blending a water-soluble antioxidant with an anionic surfactant and a nonionic surfactant-free formulation in a composition for a mouthwash containing a cationic bactericide, Or a cationic fungicide and polyvinylpyrrolidone, but not a surfactant other than a cationic fungicide This technology (see Patent Document 5) by which the composition, the antimicrobial activity of the oral composition and improve the storage stability is disclosed. However, even in these techniques, a high sterilizing power against the floating bacteria in the oral cavity is exhibited, but the sterilizing power is insufficient for the cariogenic bacteria in the biofilm and is not satisfactory.

Further, a technology for enhancing the biofilm penetration sterilization power of a non-ionic fungicide such as isopropylmethyl phenol (see Patent Literatures 6 and 7) by blending an anionic surfactant such as sodium lauryl sulfate into a liquid oral composition is proposed . In addition, the oral sterilization effect of dihydroabietic acid is increased by the use of an anionic surfactant such as sodium lauryl sulfate (see Patent Document 8). As a technique for suppressing the formation of plaques, a biosurfactant and a non- (Refer to Patent Document 9). In the case of a cationic polymer, a hydroxypyridone derivative is mixed with hydroxyethyl cellulose dimethyl dimethacrylate and / or a cationic antimicrobial agent to sterilize pathogenic bacteria in the plaque to inhibit plaque formation (Japanese Patent Application Laid-Open No. H10-21995) has been proposed in which an allyl ammonium salt is added to improve retention and suppress plaque formation.

However, these techniques are effective for periodontal pathogenic biofilms, but they are difficult to exhibit a sufficient sterilization effect against cariogenic bacteria such as Streptococcus mutans in the dental biofilm.

In addition, a composition obtained by blending polyoxyethylene hydrogenated castor oil with cetylpyridinium chloride and palmitoyl sarcosinate is exemplified in Example 2 of Patent Document 9 and Example 10 of Patent Document 10 Since these three liquids have a large number of carbon atoms in the palmytoyl group of Palmitoyl sarco cinnamium, precipitation and turbidity are generated in low-temperature preservation, and the stability of appearance can not be sufficiently secured.

Therefore, it is desired to develop a composition for liquid oral cavity which exhibits a high sterilizing power against caries bacteria in a dental caries biofilm and is excellent in appearance stability at low temperature storage.

Patent Document 1: JP-A-2006-117574

Patent Document 2: JP-A 2006-117573

Patent Document 3: JP-A-2003-113059

Patent Document 4: JP-A-7-101842

Patent Document 5: Japanese Patent Application Laid-Open No. 7-267840

Patent Document 6: JP-A 2006-069909

Patent Document 7: JP-A-2006-182663

Patent Document 8: Japanese Patent Application Laid-Open No. 2006-312588

Patent Document 9: JP-A-2003-246717

Patent Document 10: Japanese Patent Application Laid-Open No. 2002-205929

Disclosure of the Invention The present invention has been made in view of the above problems, and it is an object of the present invention to provide a biofilm for oral cavity, which is capable of rapidly penetrating a biofilm in a dental oral cavity biofilm, exhibiting a high sterilizing power against a cariogenic bacterium and suppressing the occurrence of precipitation and turbidity at low temperature storage, And a method for improving the sterilizing power of a cationic bactericide.

The inventors of the present invention have found that when cetylpyridinium chloride (A), sodium lauroyl sarcosinate (B), and (C) ethylene oxide are added in an amount of 40 to 100 moles By blending polyoxyethylene hardened castor oil at a specific ratio, the bactericide rapidly penetrates into the dental caries biofilm in the oral cavity, effectively sterilizing the dental caries bacteria, and suppressing the occurrence of precipitation and turbidity at low temperature storage And a liquid oral composition excellent in external stability can be obtained.

In this case, if the liquid oral composition is mixed with a cationic bactericidal agent having a high bactericidal activity against the cariogenic bacteria and an anionic surfactant for enhancing the penetration into the biofilm, It is expected. However, the inventors of the present invention have found that, in this case, the composite is formed by the electric interaction between the two, so that not only the sterilizing power is not sufficiently exhibited but also precipitation and turbidity estimated as a composite in low temperature storage occurs, Was damaged. Therefore, as a result of further studies, it has been found that cetylpyridinium chloride, which is a cationic fungicide, is used in combination with fungicide and sodium lauroyl sarcosine, which is used as an anionic surfactant, and the average addition mole number of ethylene oxide is 40 to 100 moles Of polyoxyethylene hardened castor oil and the combination of these components in a specific ratio makes it possible to expect that the complex formed by cetylpyridinium chloride and sodium lauroyl sarcosine rapidly penetrates into the caries biofilm , Streptococcus mutans bacteria, and the like, and it has been found that good appearance stability can be obtained without hardly causing precipitation or turbidity even when preserved at low temperature. The effect of the present invention as described above is that when cetylpyridinium chloride and sodium lauroyl sarcosinate are mixed, the two components form a complex by electrical interaction to lower the activity of the sterilizing active site of each other, But the polyoxyethylene hydrogenated castor oil having an average addition mole number of ethylene oxide of 40 to 100 moles is added to the composite at a specific ratio so as to cause precipitation or turbidity due to low solubility of the composite, And the activity of the bactericidal active site of each other is restored and the bactericidal power is sufficiently exhibited. Further, the polyoxyethylene hydrogenated castor oil can be solubilized by the surfactant action of the polyoxyethylene hydrogenated castor oil, It is thought that it is derived from that it can penetrate effectively.

The effect of the present invention as described above can be attained by using cetylpyridinium chloride and sodium lauroyl sarcosinate and polyoxyethylene hydrogenated castor oil having an average addition mole number of ethylene oxide of 40 to 100 moles In combination with other anionic surfactants or nonionic surfactants, or even when the mixing ratio of each component is outside the scope of the present invention, The purpose of

Accordingly, the present invention provides the following liquid oral composition and a method for improving the sterilizing power of a cationic bactericide.

[I]

(A) 0.01 to 0.1% by mass of cetylpyridinium chloride,

(B) 0.02 to 0.3 mass% of sodium lauroyl sarcosinate

(C) polyoxyethylene hydrogenated castor oil having an average addition mole number of ethylene oxide of 40 to 100 moles

Wherein the mass ratio of (A) / (B) is 0.3 to 3, and the mass ratio of (C) / (A) + (B) is 1.0 to 20.

[II]

A liquid oral composition according to [I], which is prepared as a detergent.

[III]

A method for improving the germicidal power of a cationic bactericide in a liquid oral composition,

(A) 0.01 to 0.1% by mass of cetylpyridinium chloride,

(B) 0.02 to 0.3 mass% of sodium lauroyl sarcosinate

(C) polyoxyethylene hydrogenated castor oil having an average addition mole number of ethylene oxide of 40 to 100 moles

, And the mass ratio of (A) / (B) is in the range of 0.3 to 3, and the mass ratio of (C) / (A) + (B) is in the range of 1.0 to 20. The cationic fungicide / RTI >

INDUSTRIAL APPLICABILITY The liquid oral composition and the method for improving the bactericidal power of the cationic bactericide of the present invention can quickly penetrate the bactericidal agent into the caries biofilm and exert an excellent sterilizing power against the caries bacteria, The appearance stability is good, and it is effective in preventing caries.

The liquid oral composition of the present invention is characterized by comprising (A) cetylpyridinium chloride, (B) sodium lauroyl sarcosine, (C) polyoxyethylene hardened castor oil having an average addition mole number of ethylene oxide of 40 to 100 mol .

The cetylpyridinium chloride as the component (A) is incorporated in an amount of 0.01 to 0.1% (mass%, the same applies hereinafter) to the entire composition, but it is preferably 0.02 to 0.05% in view of sterilizing power and appearance stability. If the blending amount is less than 0.01%, the penetration of the bactericide into the biofilm is not improved and a high sterilizing power may not be exhibited. On the other hand, if the blending amount exceeds 0.1%, the bactericide may become opaque at low temperature storage and the appearance stability may be impaired.

The blending amount of (B) lauroyl sarcosinate is preferably from 0.02 to 0.3%, more preferably from 0.05 to 0.2% from the viewpoint of sterilizing power and appearance stability. When the blending amount is less than 0.02%, the penetration of the bactericide into the biofilm is not improved and a high sterilizing power is not sufficiently exhibited in some cases. When the blending amount is more than 0.3%, precipitation or turbidity occurs in low temperature storage and appearance stability is impaired have.

The mass ratio of the component (A) / component (B) is 0.3 to 3, preferably 0.5 to 1 in terms of sterilizing power. If the ratio (A) / (B) is less than 0.3, the bactericidal power against the biofilm may not be exhibited satisfactorily. If the ratio is more than 3, precipitation or clouding may occur at low temperature storage and appearance stability may be impaired.

In the present invention, it is necessary to use (A) cetylpyridinium chloride and (B) sodium lauroyl sarcosine in a specific ratio, whereby a complex of cetylpyridinium chloride and sodium lauroyl sarcosine is formed , The complex rapidly penetrates into the dental caries biofilm, and exerts an excellent sterilizing effect against the cariogenic bacteria such as Streptococcus mutans. The use of cetylpyridinium chloride or sodium lauroyl sarcosinate alone can not achieve the object of the present invention.

As the polyoxyethylene hardened castor oil (C), one or two or more kinds of polyoxyethylene hydrogenated castor oil having an average addition mole number of 40 to 100 mol of ethylene oxide are blended. In particular, from the viewpoint of appearance stability and sterilizing power, The average addition mole number is preferably 60 to 100. When the average addition mole number is less than 40 moles, there are cases where the appearance stability is impaired during low-temperature storage or a satisfactory sterilizing power against the dough-based biofilm is not exhibited in some cases, and those exceeding 100 moles are not generally commercially available .

The blending amount of the polyoxyethylene hydrogenated castor oil as the component (C) is preferably from 0.1 to 3%, particularly from 0.2 to 2%, more preferably from 0.2 to 2%. When the content is less than 0.1%, precipitation or turbidity occurs during storage at low temperature, And when it exceeds 3%, the taste is deteriorated or the bactericidal power to the cow's tortoise bacteria is not sufficiently exhibited in some cases.

In the present invention, the total content of the component (C), the components (A) and (B) and the content of the component (B) (C) / ((A) + (B)) in terms of mass ratio is 1.0 to 20, preferably 2 to 10. When the mass ratio is less than 1.0, that is, when the content of the component (C) is less than the total amount of the components (A) and (B), precipitation or turbidity occurs during storage at low temperature, And the germicidal power to the bottom carotid gonorrhoeae is not sufficiently exhibited.

The composition for liquid oral cavity of the present invention can be used either as a type that can be used as it is without dilution during use or as a thickening agent or a mouthwash solution diluted with water at the time of use. A suitable known ingredient may be blended in accordance with the mold type. For example, a solvent, a wetting agent, a thickener, a pH adjuster, an antiseptic, a sweetener, an antioxidant, an active ingredient, a coloring agent and the like may be added. In addition, known surfactants other than the essential components may not be blended. In addition, when prepared as a detergent, the abrasive may not be blended.

As the solvent, water is generally used, but polyhydric alcohols such as propylene glycol, ethylene glycol, and polyethylene glycol, and alcohols such as lower alcohols such as ethanol and the like can also be blended. The blending amount of the alcohol is usually 0 to 30%, particularly 1 to 10%, of the whole composition.

The composition for liquid oral cavity of the present invention may be free of ethanol or may contain substantially no ethanol (that is, an ethanol content in the composition of 0.01% or less, particularly 0 to 0.0001%). Even if the composition does not substantially contain ethanol, the bactericide effectively penetrates into the caries biofilm, effectively sterilizing the caries bacteria such as Streptococcus mutans bacteria, and can suppress the occurrence of precipitation and turbidity at low temperatures have.

As the wetting agent, sugar alcohols such as glycerin, sorbitol, maltitol, lactate and the like can be blended (the blending amount is usually 0 to 20%, especially 1 to 9% of the whole composition).

As the thickening agent, xanthan gum, carrageenan, hydroxyethylcellulose, sodium alginate, polyvinyl alcohol, carboxymethylcellulose sodium and the like can be blended (the blending amount is usually 0 to 3%, particularly 0.01 to 0.5% in the total amount of the composition) .

Examples of the preservative include paraoxybenzoic acid esters such as methylparaben, ethylparaben, propylparaben and butylparaben, potassium sorbate and the like.

As the sweetening agent, xylitol, maltitol, saccharin, sodium saccharin, stevioside, aspartame and the like can be mixed.

Examples of the active ingredient include natural products such as peppermint oil, spearmint oil, eucalyptus oil, wintergreen oil, kurobu oil, time oil, sage oil, cardamon oil, rosemary oil, marjoram oil, lemon oil, nutmeg oil, lavender oil, Essential oils, and synthetic oils such as l-menthol, l-calbone, cinnamic aldehydes, orange oil, anethole, 1,8- The above-mentioned natural essential oils such as citral, camphor, borneol, pinene and spilan tall include the following components: ethyl acetate, ethyl butyrate, isoamyl acetate, hexanoal, hexenal, methyl anthranilate, Ethyl-p-menthane-3-carboxamide, menthyllactate, n-ethyl-p-menthane-3-carboxamide, Ethylene glycol-1-menthyl carbonate, Further, a combination of some of the ingredients of natural or essential oils, such as a combination of apple, banana, strawberry, blueberry, melon, pitch, pineapple, grape, musk, wine, cherry, squash, coffee, brandy and yogurt One or more flavors may be blended. The blending amount of the glue is preferably 0.00001 to 3% in the composition, and may be compounded in a range not hindering the effect of the present invention.

In addition to cetylpyridinium chloride, other active ingredients may be blended as the active ingredient. Specific examples thereof include an enzyme such as an antiinflammatory agent such as tranexamic acid and epsilon-aminocaproic acid, dextranase, amylase, protease, mutagen, lysozyme, lytic enzyme (retec enzyme), sodium fluoride, sodium monofluorophosphate, Dihydrocholesterol, copper cholinesterase, copper cholestyramine, hydrocholesterol, chlorophyll, copper, and the like, such as calcium chloride, calcium chloride, A plant extract such as chlorophyllin sodium, thyme, gold, chrysanthemum and hamamelis, copper gluconate, caropeptide, sodium polyphosphate, water-soluble inorganic phosphoric acid compound, polyvinylpyrrolidone, anti-calculus, plaque inhibitor, Aluminum lactate or the like may be added. The amount of these other active ingredients to be added is in a range not hindering the effect of the present invention.

As a coloring agent, a water-soluble coloring matter having high safety such as Blue No. 1, Green No. 3, Yellow No. 4, Red No. 105 and the like can be added.

As the pH adjusting agent, one or two or more selected from phthalic acid, phosphoric acid, citric acid, succinic acid, acetic acid, fumaric acid, malic acid and carbonic acid and their potassium salt, sodium salt and ammonium salt, ribonucleic acid and salts thereof, have. Particularly, it is preferable to use phosphoric acid and its sodium salt or a combination of citric acid and its sodium salt. The liquid oral composition of the present invention is preferably adjusted to pH 5.5 to 8.0 at 25 DEG C and therefore it is preferable to use sodium dihydrogenphosphate and sodium dihydrogenphosphate as a pH adjusting agent in the vicinity thereof or a mixture of sodium citrate and sodium citrate The combination is appropriate.

As the container, PET (polyethylene terephthalate), glass, polypropylene, and polyethylene can be used, but PET or glass is preferable from the standpoint of suppressing adsorption of the dye.

Example

Hereinafter, the present invention will be described in more detail based on Experimental Examples, Examples and Comparative Examples, but the present invention is not limited by these Examples.

In addition, the% shown in the following examples means% by mass unless specifically refused. The pH in the table was measured immediately after preparation using a pH meter (Model No. HM-30S) manufactured by DOHA Corporation, and the value after 25 minutes was 3 minutes. The parentheses in the polyoxyethylene hydrogenated castor oil show the average addition mole number of ethylene oxide.

The liquid oral composition may be prepared by mixing cetylpyridinium chloride (Wako Pure Chemical), lauroyl sarcosine sodium (natural pine-curative), polyoxyethylene (40) hardened castor oil (NIKKO CHEMICALS) (Trade name, manufactured by Nippon Shokubai Co., Ltd.), ethylene (60) hardened castor oil (manufactured by Nikko Chemicals), polyoxyethylene (80) hardened castor oil (manufactured by Nikko Chemicals), polyoxyethylene , Sodium citrate (manufactured by Fuso Chemical), sodium monohydrogenphosphate (manufactured by Taihe Pure Chemical Industries), sodium dihydrogenphosphate (manufactured by Taihei Chemical Industry Co., Ltd.), xylitol (rocket holic acid), sorbitol (API), butylparaben (API), and saccharin sodium (manufactured by Nippon Kayaku Co., Ltd.)), polyethylene glycol (manufactured by Daiichi Kogyo Seiyaku Co., Ltd.), propylene glycol Manufactured by Daito Chemical Co., Ltd.), glycerin (85%, manufactured by Sakamoto Pharmaceutical Industry Co., Ltd.) The volume (Stella Paget Chemie), aspartame (Ajinomoto claim), DEX trad xylanase (Temple and Cemetery of Confucius and the Kong Family Mansion in Qufu the best), carrageenan (Samjeong agent) was used. The dyes of the compositions shown in Table 3 below were used as the dyes.

In addition, in the preparation of the comparative example, in addition to the components used in the above-mentioned Examples, sodium lauryl sulfate (manufactured by Dongfang Chemical Industries), palmitoyl sarcosine sodium (manufactured by Nikko Chemicals), poly Oxyethylene (20) hardened castor oil (manufactured by Nikko Chemicals) and polyoxyethylene (40) cetyl ether (made by Nippon Emulsion) were used.

[Experimental Example 1]

A liquid oral composition (cedar) having the composition shown in Tables 1 and 2 was prepared by the routine method, and the following evaluation was made using the composition as a sample.

Penetration effect of cetylpyridinium chloride on dental biofilm

30 g of trypticase soy broth (manufactured by Difco) was dissolved in 1 L of purified water and 10 g of sucrose (manufactured by Wako Pure Chemical Industries, Ltd.) was used as a culture solution. 2 mL of the culture solution inoculated with Streptococcus mutans ATCC 10449 Co., Ltd. as a dormant strain of the caries bacterium was placed in a glass small test tube having a diameter of 13 mm x 150 mm and placed on a test tube (Sanwakaken, 13 mm) The cells were incubated at 37 ° C under anaerobic conditions (5% by volume carbonic acid gas, 95% by volume nitrogen) for 18 hours to form and adhere a biofilm.

The culture medium in the test tube was discarded, and the formed biofilm was adjusted to pH 4.5 with phosphate buffer (8.8 g of sodium chloride and 1.56 g of sodium dihydrogenphosphate dihydrate dissolved in 1 L of purified water, adjusted to pH 4.5 with 1 N aqueous sodium hydroxide solution 1 < / RTI > After the buffer solution was discarded, 0.5 mL of the sample shown in Tables 1 and 2 was added and immersed for 30 seconds. Thereafter, the sample solution was discarded and the biofilm was dispersed by ultrasonication (using US-300, 200,, 10 seconds) with 2 mL of sterile physiological saline. (Internal standard material solution) obtained by dissolving 0.1 g of 4-octylphenyl salicylate (manufactured by Tokyo Chemical Industry Co., Ltd.) as an internal standard substance in 5 L of ethanol (99.5%, manufactured by Kanto Kagaku) was added to the solution, and the mixture was filtered through a 0.45 μm membrane filter , And the amount of cetylpyridinium chloride that penetrated the biofilm was determined by measuring the filtrate by liquid chromatography (sample injection amount: 40 μL).

PU-980 manufactured by Nippon Gosei Co., Ltd., sample introduction part: AS-950 manufactured by Nippon Gosei Co., Ltd., detector: UV-970 manufactured by Nippon Gosei Co., Ltd. (Set at 355 ° C): CO-966, manufactured by Nippon Gosei Co., Ltd. Column: GL Scientific Co., Ltd. Inertsil ODS-2 (set at a wavelength of 265 nm) Recording apparatus: Chromatocorder 21J, Mm < / RTI > x 150 mm). In addition, as a standard solution, 2 mL of a solution obtained by dissolving 0.1 g of cetylpyridinium chloride (Wako Pure Chemical) in 200 mL of a mobile phase and diluting at 125 times (volume ratio) in a mobile phase was taken and 1 mL of the internal standard solution was added The solution was similarly measured by liquid chromatography (sample injection amount: 40 mu L).

From the peak area ratio of cetylpyridinium chloride / internal standard material, the amount of cetylpyridinium chloride penetrated into the biofilm was calculated using the following equation, and the penetration effect of the fungicide was evaluated from the following criteria.

The results are shown in Tables 1 and 2.

[Equation 1]

Amount of cetylpyridinium chloride (㎍) penetrated =

Criteria for the penetration effect of bactericides

&Amp; cir &: The amount of cetylpyridinium chloride penetrated was 40 mu g or more

○: The amount of cetylpyridinium chloride that penetrated was 30 μg or more and less than 40 μg

?: The amount of cetylpyridinium chloride penetrated was 20 占 이상 to 30 占 퐂

X: Less than 20 占 퐂 of cetylpyridinium chloride penetrated

[Experimental Example 2]

Sterilization effect on Streptococcus mutans bacteria in biofilm of duckweed

30 g of trypticase soy broth (manufactured by Difco) was dissolved in 1 L of purified water and 10 g of sucrose (manufactured by Wako Pure Chemical Industries, Ltd.) was used as a culture solution. Streptococcus mutans ATCC 10449 strain was inoculated as a dormant brood of wheat germ, and a hydroxyapatite (HA) plate (Asahi Optics) having a diameter of 7 mm and a thickness of 3.5 mm was placed in the culture medium and incubated under anaerobic conditions (5 volume% Carbon dioxide gas, 95% by volume nitrogen) for 18 hours to form a biofilm.

The HA plate with attached biofilm was taken out from the culture solution. This HA plate was dissolved in 1 L of purified water and adjusted to pH 4.5 with 1 N sodium hydroxide solution), 100 ml of a phosphate buffer solution (pH 8.8, sodium chloride 8.8 g and sodium dihydrogenphosphate 1.56 g) And washed in the contained beaker.

Next, the HA plate was immersed in 10 mL of the sample shown in Tables 1 and 2 for 30 seconds, immersed in 2 mL of the phosphate buffer solution adjusted to pH 4.5, and incubated for 3 hours in a 37 DEG C thermostat (Yamato Scientific IS400) Respectively. Next, the HA plate adhered to the biofilm was taken out, and the biofilm was dispersed by ultrasonication (US-300, 200 ㎂, 10 seconds) using 2 mL of sterile physiological saline. 45 g of Mitus salivarius agar (manufactured by Difco) and 25 g of sucrose (manufactured by Wako Pure Chemical Industries, Ltd.) diluted with sterilized physiological saline at a dose ratio of 10, 100, 1,000, 10,000 and 100,000, Was dissolved in 500 mL of purified water and then 50 L L was plated on an agar plate which had been sterilized by heating and then cultured at 37 째 C for 3 days. The grown colonies were counted, and the number (cfu) of the remaining Streptococcus mutans bacteria was calculated and determined according to the following criteria.

The results are shown in Tables 1 and 2.

Criteria for determining biofilm sterilization effect

?: The number of living cells was less than 106

&Amp; cir &

DELTA: Number of live cells is 107 or more and less than 108

X: The number of viable cells was 108 or more

[Experimental Example 3]

Evaluation of appearance stability

450 mL of the sample shown in Tables 1 and 2 was filled in a colorless transparent PET container (polyethylene terephthalate container, Yoshino Kogyo Co., Ltd.) having a volume of 500 mL, and the mixture was kept at 5 ° C in a thermostat bath (MPR- Was visually judged according to the following criteria for appearance stability after storage for 1 month.

The results are shown in Tables 1 and 2.

Apparent Stability Evaluation Standard

⊚: There is no precipitation or turbidity, and it is transparent.

○: Very small floating matter is recognized at the time of shaking, but it is transparent and there is no problem.

?: Slight precipitation and turbidity are recognized.

X: Significant sedimentation and turbidity are recognized.

The results of Tables 1 and 2 show that Comparative Example 1 using (A) triclosan which is widely used as a fungicide instead of (A) cetylpyridinium chloride, (B) Comparative Example 2 using sodium laurylsulfate instead of sodium lauroyl sarcosine , Comparative Example 3 using polyoxyethylene (20) hardened castor oil as a nonionic surfactant, Comparative Example 4 using polyoxyethylene (40) cetyl ether, and Component (A) (A) Comparative Examples 7 and 8 in which the content of cetylpyridinium chloride was out of the range of 0.01 to 0.1%, (B) Comparison in which the sodium lauroyl sarcosinate content was out of the range of 0.02 to 0.3% Comparative Examples 11 and 12 in which the mass ratios of Examples 9 and 10 and (C) / ((A) + (B)) were out of the range of 1.0 to 20 showed poor permeability of the bactericide in the caries biofilm, Or the appearance stability is deteriorated. Also, in Comparative Example 13 in which palmitoyl sarcosine sodium was blended instead of sodium lauroyl sarcosinate (B), precipitation and turbidity occurred at low temperature storage, and appearance stability was not sufficiently secured.

In contrast to these, the liquid oral compositions (Examples 1 to 16) of the present invention effectively infiltrated the fungicide into the dormant biofilm, exhibited high sterilizing power, and caused the occurrence of precipitation and turbidity in low-temperature storage And excellent in appearance stability. ≪ tb > < TABLE >

[Table 1]

[Table 2]

[Table 3]

[Table 4]

All parts in the table are parts by mass (the same applies hereinafter).

[Table 5]

[Table 6]

[Table 7]

[Table 8]

[Table 9]

Claims (3)

(A) 0.01 to 0.1% by mass of cetylpyridinium chloride,
(B) 0.02 to 0.3 mass% of sodium lauroyl sarcosinate
(C) 0.1 to 3% by mass of polyoxyethylene hydrogenated castor oil having an average addition mole number of ethylene oxide of 40 to 100 moles,
Wherein the mass ratio of (A) / (B) is 0.3 to 3, and the mass ratio of (C) / ((A) + (B)) is 1.0 to 20. The method of claim 1, wherein
A transparent liquid oral composition for preventing caries, which is prepared as a salve. A method for improving the biofilm sterility of a cationic bactericide in a transparent liquid oral composition,
(A) 0.01 to 0.1% by mass of cetylpyridinium chloride,
(B) 0.02 to 0.3 mass% of sodium lauroyl sarcosinate
(C) 0.1 to 3% by mass of polyoxyethylene hardened castor oil having an average addition mole number of ethylene oxide of 40 to 100 moles,
Wherein the mass ratio of (A) / (B) is 0.3 to 3, and the mass ratio of (C) / ((A) + (B)) is in the range of 1.0 to 20. How to improve.